CN1120030A - Synthesizing efficient cement water reducing agent by using waste phenol dregs oil refinery - Google Patents
Synthesizing efficient cement water reducing agent by using waste phenol dregs oil refinery Download PDFInfo
- Publication number
- CN1120030A CN1120030A CN 94104749 CN94104749A CN1120030A CN 1120030 A CN1120030 A CN 1120030A CN 94104749 CN94104749 CN 94104749 CN 94104749 A CN94104749 A CN 94104749A CN 1120030 A CN1120030 A CN 1120030A
- Authority
- CN
- China
- Prior art keywords
- waste
- oil refinery
- water reducing
- reducing agent
- phenol dregs
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/001—Waste organic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The efficient water-reducing agent for concrete used for construction of runway, dam or high-grade highway is prepared from waste phenolic dregs from oil refinery through such technological steps as sulfonating the waste phenolic dregs using concentrated sulfuric acid, condensation, neutralization, and spray drying to obtain powder product, and contains mainly alkylphenol-sulfonic acid-aromatic fused ring compound, condensate of formaldehyde sulfonate or amino formaldehyde and sodium sulfate. When it is mixed with concrete by 0.05-0.1 percentage, the water-reducing rate is up to 15-20%.
Description
The invention belongs to the production method of material of construction cement additive, specifically utilize the method for the waste phenol dregs synthesizing efficient cement water reducing agent that refinery emits.
In petroleum refining process, often there is a large amount of useless phenol mixtures to discharge.Its fundamental component is phenol, cresols, xylenol and other aromatic fused ring compounds.This industrial residue is water insoluble, poisonous, during heating in the pitch shape, only reclaim a part at present and be used for preparing the poor efficiency agricultural chemicals, poor because of the Biodegradable of phenol, so environment is caused severe contamination, if directly be disposed in the rivers, then pollution is more abominable.The objective of the invention is to propose a kind of method of utilizing the waste phenol dregs oil refinery synthesizing efficient cement water reducing agent.The discharging of using this method not only can solve waste phenol dregs oil refinery, and control pollution problems, and can obtain the important cement additive of construction sector---efficient cement water reducing agent again.
At present, commercially available efficient cement water reducing agent, adopt naphthalene is raw material more, thereby the production cost height.The present invention directly adopts waste phenol dregs oil refinery, utilizes operations such as sulfonation, condensation, neutralization, spraying drying, makes efficient cement water reducing agent.This water reducer is a chocolate brown powder, when add in the concrete cement amount 0.4% the time, water-reducing rate can reach 15～20%.
The main process and the chemical reaction of this technology are as follows:
1, sulfonation reaction
For explaining conveniently, above-mentioned reaction formula the right is with PhSO
3H represents.
2, condensation reaction:
Or:
3, neutralization reaction:
4, spraying drying forms powder-like product
Implementation process of the present invention is as follows:
With in the oil waste phenol dregs, adding people's sulfuric acid material in 1～5 hour, be warming up to 60～150 ℃ after adding, be incubated 2～8 hours, in 40～100 ℃ temperature range, add people's formaldehyde gradually, the reinforced time was controlled at 1～5 hour, after formaldehyde adds, can further add properties-correcting agent, and under uniform temp, keep reaction 1～10 hour, until reacting completely, be cooled to 30～50 ℃ then, add the people NaOH aqueous solution gradually, make PH=7～9, the product of formation after filtration, spraying drying and make tan powder-product.
In sulfonation reaction, the concentration of the vitriol oil is controlled at 98%, and sulfuric acid should be controlled at the ratio of oil waste phenol dregs: 1.0～3.0: 1.
In condensation reaction, waste phenol dregs: formaldehyde: aminocompound should be controlled at 1: 0.05～0.2: 0～0.3.
Because starting raw material waste phenol dregs oil refinery of the present invention is the mixture of a kind of phenol, cresols, xylenol and other condensed nucleus aromatic compounds.So the efficient cement water reducing agent major ingredient that makes is alkyl phenol sulfonic, aromatic fused ring sulfonic acid and formaldehyde polycondensate and sodium sulfate and aminoresin modifier and sodium sulfate.During use when add cement amount 0.3～0.6% the time, water-reducing rate reaches 15～20%.So be a kind of high efficiency water reducing agent.
Embodiment:
By 98% vitriol oil: the oil waste phenol dregs: the weight ratio of formaldehyde=1.75: 1: 0.2, taking by weighing the 500kg waste phenol dregs puts in the people 2000L enamel still, be heated to 70 ℃, drip the 875kg98% vitriol oil, be warming up to 90～120 ℃ after dripping, be incubated 5 hours, be cooled to 50 ℃ then,, dropwise the back and be warming up to 105 ℃ with 1 hour with the formaldehyde solution that slowly dripped 100kg 37% in 1 hour, be incubated 5 hours, treat that the material thickness can flow, during formaldehydeless flavor, add the neutralization of NaOH solution, make pH=7～9, carry out concentrate drying then, get the chocolate brown powder product.
Technology of the present invention is simple, and is with short production cycle, and raw material is cheap and easy to get, and prepared water reducer can significantly improve concrete performance, saves cement consumption, the reduction of erection time, improves construction quality.
Claims (4)
1, a kind of method of utilizing waste phenol dregs oil refinery to prepare efficient cement water reducing agent.The technical process of this method comprises: waste phenol dregs oil refinery → concentrated acid sulfonation → condensation → neutralization → spraying drying → formation chocolate brown powder product → packing.Its principal character is, under 60～150 ℃ condition, adds people's vitriol oil with suitable speed, and reinforced 1～5 hour time is behind reinforced the end, in 60～150 ℃ of insulations 2～8 hours down.Under 30～100 ℃ of conditions, add formaldehyde then, be warming up to 70～150 ℃ and continue reaction 1-10 hour.When treating material, can add aminocompound in right amount, until reacting completely than thickness.Reaction product is neutralized to pH=7-9 with caustic soda.At last, spraying drying, finished product packing.
2, described by claim 1, utilize waste phenol dregs oil refinery to prepare the method for efficient cement water reducing agent.Its principal character is, during sulfonation, the weight ratio of 98% vitriol oil and waste phenol dregs oil refinery is 1.0～3.0: 1, during condensation reaction, and waste phenol dregs: 37% formaldehyde: aminocompound=1: 0.05～0.3: 0～0.3.
3, by claim 1, used aminocompound is urea, trimeric cyanamide and derivative thereof.
4, by the described method of claim 1, utilize other industrial waste phenol dregs, as the gossypol waste residue, synthesizing efficient cement water reducing agents such as refining dihydroxyphenyl propane waste residue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94104749 CN1120030A (en) | 1994-05-13 | 1994-05-13 | Synthesizing efficient cement water reducing agent by using waste phenol dregs oil refinery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94104749 CN1120030A (en) | 1994-05-13 | 1994-05-13 | Synthesizing efficient cement water reducing agent by using waste phenol dregs oil refinery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1120030A true CN1120030A (en) | 1996-04-10 |
Family
ID=5031735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94104749 Pending CN1120030A (en) | 1994-05-13 | 1994-05-13 | Synthesizing efficient cement water reducing agent by using waste phenol dregs oil refinery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1120030A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089733C (en) * | 1998-10-21 | 2002-08-28 | 四川联合大学 | Efficient water-reducing agent for high-strength concrete and its preparing process and use |
| CN1091434C (en) * | 1999-05-19 | 2002-09-25 | 四川大学 | Solid concrete water reducing agent and its preparation |
| CN103254380A (en) * | 2013-05-10 | 2013-08-21 | 济南融祺建材有限公司 | Production method of melamine high-efficiency water reducer |
| CN105778024A (en) * | 2016-03-10 | 2016-07-20 | 安徽鑫固环保股份有限公司 | Waste petroleum phenolic residue modified sulfamate high-efficiency water reducing agent and preparation method thereof |
| CN107043446A (en) * | 2017-04-19 | 2017-08-15 | 邵启明 | A kind of waste liquid modified high efficiency water reducing agent of carboxylic acid of 9 Fluorenone 2 |
| CN107954626A (en) * | 2017-12-05 | 2018-04-24 | 山东理工大学 | The preparation method of biomass-based water-reducing agent |
| CN108753333A (en) * | 2018-08-15 | 2018-11-06 | 山西新元太生物科技股份有限公司 | A kind of device that phenol slag recycling is generated to coal tar pitch |
| CN110813983A (en) * | 2019-10-31 | 2020-02-21 | 金能科技股份有限公司 | Method and device for recycling solid waste phenol residues produced in alkylphenol production process |
-
1994
- 1994-05-13 CN CN 94104749 patent/CN1120030A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089733C (en) * | 1998-10-21 | 2002-08-28 | 四川联合大学 | Efficient water-reducing agent for high-strength concrete and its preparing process and use |
| CN1091434C (en) * | 1999-05-19 | 2002-09-25 | 四川大学 | Solid concrete water reducing agent and its preparation |
| CN103254380A (en) * | 2013-05-10 | 2013-08-21 | 济南融祺建材有限公司 | Production method of melamine high-efficiency water reducer |
| CN103254380B (en) * | 2013-05-10 | 2015-05-06 | 济南融祺建材有限公司 | Production method of melamine high-efficiency water reducer |
| CN105778024A (en) * | 2016-03-10 | 2016-07-20 | 安徽鑫固环保股份有限公司 | Waste petroleum phenolic residue modified sulfamate high-efficiency water reducing agent and preparation method thereof |
| CN107043446A (en) * | 2017-04-19 | 2017-08-15 | 邵启明 | A kind of waste liquid modified high efficiency water reducing agent of carboxylic acid of 9 Fluorenone 2 |
| CN107954626A (en) * | 2017-12-05 | 2018-04-24 | 山东理工大学 | The preparation method of biomass-based water-reducing agent |
| CN107954626B (en) * | 2017-12-05 | 2020-08-21 | 山东理工大学 | Preparation method of biomass-based water reducing agent |
| CN108753333A (en) * | 2018-08-15 | 2018-11-06 | 山西新元太生物科技股份有限公司 | A kind of device that phenol slag recycling is generated to coal tar pitch |
| CN110813983A (en) * | 2019-10-31 | 2020-02-21 | 金能科技股份有限公司 | Method and device for recycling solid waste phenol residues produced in alkylphenol production process |
| CN110813983B (en) * | 2019-10-31 | 2021-09-17 | 金能科技股份有限公司 | Method and device for recycling solid waste phenol residues produced in alkylphenol production process |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |